CN111856138A - Device and method for measuring resistivity of micro-scale metal sample - Google Patents

Device and method for measuring resistivity of micro-scale metal sample Download PDF

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Publication number
CN111856138A
CN111856138A CN202010610197.6A CN202010610197A CN111856138A CN 111856138 A CN111856138 A CN 111856138A CN 202010610197 A CN202010610197 A CN 202010610197A CN 111856138 A CN111856138 A CN 111856138A
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CN
China
Prior art keywords
substrate
measuring
resistivity
sample
test electrode
Prior art date
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Pending
Application number
CN202010610197.6A
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Chinese (zh)
Inventor
傅思伟
叶芳
李田
齐文艳
张迅达
陈韶瑜
周连升
管森森
甘智勇
于金山
文黎
温力
李庆钊
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State Grid Corp of China SGCC
State Grid Tianjin Electric Power Co Ltd
Electric Power Research Institute of State Grid Tianjin Electric Power Co Ltd
Original Assignee
State Grid Corp of China SGCC
State Grid Tianjin Electric Power Co Ltd
Electric Power Research Institute of State Grid Tianjin Electric Power Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by State Grid Corp of China SGCC, State Grid Tianjin Electric Power Co Ltd, Electric Power Research Institute of State Grid Tianjin Electric Power Co Ltd filed Critical State Grid Corp of China SGCC
Priority to CN202010610197.6A priority Critical patent/CN111856138A/en
Publication of CN111856138A publication Critical patent/CN111856138A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01RMEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R27/00Arrangements for measuring resistance, reactance, impedance, or electric characteristics derived therefrom
    • G01R27/02Measuring real or complex resistance, reactance, impedance, or other two-pole characteristics derived therefrom, e.g. time constant
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01RMEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R3/00Apparatus or processes specially adapted for the manufacture or maintenance of measuring instruments, e.g. of probe tips

Abstract

The invention relates to a device and a method for measuring the resistivity of a micro-scale metal sample, wherein a test electrode and a temperature measuring electrode are firstly manufactured on a substrate, the sample is placed on the substrate and is connected with the test electrode, and the test electrode is connected with a four-wire method resistance measuring circuit; and (3) placing the substrate on a heating table, placing the substrate and the heating table into a vacuum chamber, and drawing a curve of the change relation of the resistivity with the temperature by adjusting the temperature. The invention can measure the resistivity of samples with various shapes and smaller sizes, and selects different processes for depositing electrodes according to the size and the shape of the samples.

Description

Device and method for measuring resistivity of micro-scale metal sample
Technical Field
The invention belongs to the field of resistivity test of metal samples, relates to a four-wire method technology, and particularly relates to a device and a method for measuring the resistivity of a micro-scale metal sample based on a four-wire method.
Background
At present, a lot of methods and devices are used for measuring the resistivity of a metal sample, but most of the methods are directed to a sample with a large size and have certain requirements on the shape, thickness, surface state and the like of the sample, while the methods are less directed to a micro-scale metal sample, and the methods are also directed to a method for measuring the size of the sample in millimeter level and have the same requirements on the shape of the sample. In order to measure the resistivity of samples with various shapes and smaller sizes, a new method needs to be developed for measurement.
Four wire connection as shown in fig. 1, two requirements are connected: each test point is provided with an excitation line and a detection line which are strictly separated to form independent loops respectively; at the same time, the detection line must be connected to a test loop with very high input impedance, so that the current flowing through the detection line is very small and is approximately zero. The excitation line is a current supply circuit, the detection line is a voltage measurement circuit, and the current circuit and the voltage circuit are independent. The two terminals of the current supply loop and the two terminals of the voltage measuring loop are four terminals in total, so the test is called four-wire test. V1I 1 xR (because I2 (small current) is multiplied by small resistance to obtain smaller voltage drop), because the internal impedance of the voltmeter is very high (m omega level), and is far greater than the feeder resistances R3 and R4 (omega level) of the voltage measuring loop, almost all the current flows through R, the current I2 flowing through the voltmeter is almost zero, the measured voltage is almost the voltage drop of R, the feeder resistance can be completely ignored, the measured R is almost similar to R, therefore, the tiny resistance value of the measured resistance can be accurately measured, and the measuring accuracy of the four-wire test can reach m omega level. In the four-terminal test (fig. 2), the current supply circuit and the voltage measurement circuit are independent (4 terminals are counted as the terminal of the current supply circuit 2 and the terminal of the voltage measurement circuit 2), and because the internal impedance of the voltage measurement meter is very high, the flat cable impedance, the contact impedance and the internal impedance in the voltage measurement circuit can be ignored, so that the tiny resistance value of the measured resistor can be accurately measured.
The advantage of the four-wire method is that not only the lead resistance and the contact resistance are eliminated, but also the influence of the thermal electromotive force can be greatly reduced. Because the current terminal is a heating source, but under the action of the constant current after the current terminal is separated, how large a resistor is connected in series to the bottom, even a battery is connected in series, the resistor is constant current, and therefore the current terminal can also be used in common. On the other hand, the two voltage terminals do not generate heat because no current flows, and the distance between the two voltage terminals and the current terminal generating heat is kept constant, so that the heat conduction can be reduced, and the wiring terminal can adopt low-heat.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for measuring the resistivity of a micro-scale metal sample based on a four-wire method, which can measure the resistivity of samples with various shapes and smaller sizes.
The technical scheme adopted by the invention for solving the technical problem is as follows:
a device for measuring the resistivity of a micro-scale metal sample comprises a substrate, wherein a graphical test electrode is arranged on the substrate, a sample to be measured is arranged on the substrate and is connected with the test electrode, and the test electrode is connected with a resistance measuring circuit.
Moreover, the patterned test electrode is manufactured by adopting a photoetching method or a method of combining a metal physical mask plate with physical vapor deposition or an ink-jet printing method.
Furthermore, the apparatus includes a heater for changing the temperature of the sample. The heater is disposed below the substrate.
Moreover, the device also comprises a vacuum chamber for avoiding sample oxidation, and the substrate is arranged in the vacuum chamber.
And the substrate is provided with a temperature measuring resistor, and the temperature measuring electrode is connected with a temperature display and can display real-time temperature.
Moreover, a cover plate is mounted above the base plate.
A method for measuring the resistivity of a micro-scale metal sample based on a four-wire method comprises the steps of firstly manufacturing a test electrode on a substrate, placing the sample on the substrate, connecting the sample with the test electrode, connecting the test electrode with a four-wire method resistance measuring circuit, and continuously measuring the resistivity of the sample.
A method for measuring the resistivity of a micro-scale metal sample based on a four-wire method comprises the steps of firstly manufacturing a test electrode and a temperature measuring electrode on a substrate, placing the sample on the substrate and connecting the sample with the test electrode, wherein the test electrode is connected with a four-wire method resistance measuring circuit; and (3) placing the substrate on a heating table, placing the substrate and the heating table into a vacuum chamber, and drawing a curve of the change relation of the resistivity with the temperature by adjusting the temperature.
The invention has the advantages and positive effects that:
1. the invention can measure the resistivity of samples with various shapes and smaller sizes, and selects different processes for depositing electrodes according to the size and the shape of the samples.
2. The invention is provided with the heating table, and can measure the relation of the conductivity of the sample along with the temperature change in situ.
3. The temperature measuring electrode is deposited on the substrate, so that the actual temperature of the sample can be accurately measured, and the measurement accuracy is improved.
4. The invention adopts a four-wire method to measure the resistance, can avoid the influence of contact resistance and line resistance on the test result and improve the test accuracy.
5. The present invention can manufacture a vacuum degree up to 10 by using molecular pump set-4And the Pa vacuum test environment avoids the sample from being oxidized or damaged due to the reaction of the sample and the gas in the air in the test process.
Drawings
FIG. 1 is a circuit diagram of a four-wire method for measuring resistance;
FIG. 2 is a schematic diagram of resistance measurement by a four-wire method;
FIG. 3 is a schematic view of the structure of the device of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments, which are illustrative only and not limiting, and the scope of the present invention is not limited thereby.
The device for measuring the resistivity of the micro-scale metal sample comprises a substrate 8, a heating table 9 and a vacuum chamber 4, wherein the vacuum chamber is connected with a molecular pump 3. A heating table and a substrate are arranged in a vacuum chamber, and patterned electrodes are arranged on the upper surface of the substrate and comprise a test electrode 2 and a temperature measuring electrode 7. The sample 1 to be tested is connected with the test electrode, the test electrode is connected with the resistance measuring circuit, and the temperature measuring electrode is connected with the temperature display, so that the real-time temperature can be displayed.
A cover plate 5 is arranged above the base plate, four limiting columns 6 are symmetrically arranged at four corners of the bottom surface of the cover plate, and four limiting holes are arranged at the positions, corresponding to the four limiting columns, of the four corners of the base plate.
The heating table is used for heating a test original and a sample, can be used for testing the resistivity of the sample at different temperatures, and draws a change relation curve of the resistivity along with the temperature.
The temperature measuring electrode accurately records the actual temperature of the sample by measuring the resistance of the electrode by utilizing the linear relation of the resistance of the electrode material along with the change of the temperature.
The vacuum chamber is used for preventing the sample from being oxidized in the temperature rising process.
The substrate is made of insulating high-temperature-resistant materials such as mica, quartz, polyether-ether-ketone and the like or high-temperature-resistant materials with passivation layers on the surfaces such as silicon oxide sheets and the like, and the patterned electrode is manufactured on the substrate so as to achieve the purpose of measuring the miniaturized metal sample.
The patterned electrode material can be prepared by the following methods:
1. the patterned template is manufactured by common ultraviolet lithography or electron beam exposure lithography, and then metal materials such as Au, Pt and the like are deposited by using a physical vapor deposition (such as magnetron sputtering and electron beam evaporation) method. The minimum electrode width can be up to 2 microns (ultraviolet lithography) and 200nm (electron beam exposure), and the minimum in-plane dimension of the sample can be measured to be 100 microns by 10 microns.
2. The electrode is prepared by combining a metal physical mask plate and physical vapor deposition, the minimum width of the electrode can reach 50 mu m, and the minimum size of the measurable sample plane can reach 1mm 20 mu m.
3. And printing conductive ink on the insulating substrate by using an ink-jet printing technology, wherein the conductive ink is made of Ag-doped conductive solution. The minimum electrode width can reach 100 microns, and the minimum size of the sample plane can be measured to be 2mm by 20 microns.
A method for measuring the resistivity of a micro-scale metal sample based on a four-wire method comprises the steps of firstly manufacturing a test electrode and a temperature measuring electrode on a substrate; placing a sample on a substrate, connecting the sample with a test electrode, and connecting the test electrode with a four-wire resistance measurement circuit; the substrate is placed on the heating table, the substrate and the heating table are placed in a vacuum chamber, the resistivity of the sample is continuously measured, and a change relation curve of the resistivity along with the temperature can be drawn by adjusting the temperature. The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept, and these changes and modifications are all within the scope of the present invention.

Claims (8)

1. An apparatus for measuring the resistivity of a microscale metal sample, comprising: the device comprises a substrate, wherein a graphical test electrode is arranged on the substrate, a sample to be tested is arranged on the substrate and is connected with the test electrode, and the test electrode is connected with a resistance measuring circuit.
2. The apparatus for measuring resistivity of a micro-scale metal sample according to claim 1, wherein: the patterned test electrode is manufactured by adopting a photoetching method or a method of combining a metal physical mask plate with physical vapor deposition or an ink-jet printing method.
3. The apparatus for measuring resistivity of a micro-scale metal sample according to claim 1, wherein: the device also comprises a heater for changing the temperature of the sample, wherein the heater is arranged below the substrate and is controlled by the temperature controller.
4. The apparatus for measuring resistivity of a micro-scale metal sample according to claim 1 or 3, wherein: the device also comprises a vacuum chamber for avoiding sample oxidation, and the substrate is arranged in the vacuum chamber.
5. The apparatus for measuring resistivity of a micro-scale metal sample according to claim 1 or 2, wherein: the substrate is provided with a temperature measuring resistor, and the temperature measuring electrode is connected with a temperature display.
6. The apparatus for measuring resistivity of a micro-scale metal sample according to claim 1 or 3, wherein: a cover plate is mounted above the base plate.
7. A method for measuring the resistivity of a micro-scale metal sample based on a four-line method is characterized by comprising the following steps: firstly, a test electrode is manufactured on a substrate, a sample is placed on the substrate and is connected with the test electrode, and the test electrode is connected with a four-wire resistance measuring circuit to continuously measure the resistivity of the sample.
8. A method for measuring the resistivity of a micro-scale metal sample based on a four-line method is characterized by comprising the following steps: firstly, manufacturing a test electrode and a temperature measuring electrode on a substrate, placing a sample on the substrate, connecting the sample with the test electrode, and connecting the test electrode with a four-wire resistance measuring circuit; and (3) placing the substrate on a heating table, placing the substrate and the heating table into a vacuum chamber, and drawing a curve of the change relation of the resistivity with the temperature by adjusting the temperature.
CN202010610197.6A 2020-06-30 2020-06-30 Device and method for measuring resistivity of micro-scale metal sample Pending CN111856138A (en)

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CN202010610197.6A CN111856138A (en) 2020-06-30 2020-06-30 Device and method for measuring resistivity of micro-scale metal sample

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Application Number Priority Date Filing Date Title
CN202010610197.6A CN111856138A (en) 2020-06-30 2020-06-30 Device and method for measuring resistivity of micro-scale metal sample

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1186411A (en) * 1996-09-30 1998-07-01 赫罗伊斯传感器-奈特股份有限公司 Manufacture of printed circuit board with contacting area, and connecting method and use
CN101692111A (en) * 2009-10-13 2010-04-07 中国科学院上海光学精密机械研究所 Device and method for testing resistivity of tin dioxide electrode
CN102539932A (en) * 2010-10-19 2012-07-04 恩德莱斯和豪瑟尔测量及调节技术分析仪表两合公司 Conductivity sensor
CN107765092A (en) * 2016-08-22 2018-03-06 兴亚株式会社 Probe unit
CN109581060A (en) * 2018-12-20 2019-04-05 云南大学 A method of in uneven temperature test material conductivity off field

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1186411A (en) * 1996-09-30 1998-07-01 赫罗伊斯传感器-奈特股份有限公司 Manufacture of printed circuit board with contacting area, and connecting method and use
CN101692111A (en) * 2009-10-13 2010-04-07 中国科学院上海光学精密机械研究所 Device and method for testing resistivity of tin dioxide electrode
CN102539932A (en) * 2010-10-19 2012-07-04 恩德莱斯和豪瑟尔测量及调节技术分析仪表两合公司 Conductivity sensor
CN107765092A (en) * 2016-08-22 2018-03-06 兴亚株式会社 Probe unit
CN109581060A (en) * 2018-12-20 2019-04-05 云南大学 A method of in uneven temperature test material conductivity off field

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